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Master's Dissertation
DOI
https://doi.org/10.11606/D.85.2008.tde-27082009-163738
Document
Author
Full name
Ivanildo Antonio dos Santos
Institute/School/College
Knowledge Area
Date of Defense
Published
São Paulo, 2008
Supervisor
Committee
Ranieri, Izilda Marcia (President)
Baldochi, Sonia Licia
Hernandes, Antonio Carlos
Title in Portuguese
Estudo das soluções sólidas de LiGd1-xLuxF4 visando o crescimento de cristais.
Keywords in Portuguese
Crescimento de cristais
Fluoretos
Terras raras
Abstract in Portuguese
No presente trabalho o comportamento de fusão de soluções sólidas do tipo LiGd1-xLuxF4 foram estudadas utilizando a técnica de fusão zonal, tendo em vista o desenvolvimento de novas matrizes para lasers do estado sólido. Os cristais de composição LiGd0,5Lu0,5F4 foram sistematicamente investigados. A caracterização física e química dos lingotes obtidos mostrou que este composto apresenta fusão incongruente. Posteriormente foram estudadas algumas composições do LiGd1-xLuxF4 (x = 0,60; 0,65 e 0,75), para estabelecer a composição a partir da qual começa a formação de compostos congruentes no pseudosistema LiGdF4-LiLuF4. A caracterização dos lingotes, utilizando-se as técnicas de microscopia eletrônica de varredura, espectrometria de energia dispersiva e difração de raios X, permitiu determinar que o LiGd1-xLuxF4 torna-se congruente a partir de valores de x em torno de 75 mol%. Nesta etapa do trabalho, as sínteses e os processos de fusão zonal foram realizados sob atmosfera reativa de HF, para garantir a obtenção de compostos de alta pureza. Dois monocristais de composições nominais de LiGd0,25Lu0,75F4 e LiGd0,232Lu0,75Nd0,018F4 foram crescidos com sucesso utilizando-se o método de Czochralski, sob atmosfera de Ar + CF4. A partir dos dados de concentração dos constituintes, obtidos por ICP-OES, para o cristal do dopado com neodímio, verificou-se que o íon Lu e o Gd apresentam variação de composição ao longo do cristal, sendo que a incorporação do íon Nd na rede compete com a do Gd. O valor médio calculado para o coeficiente de segregação do Nd nesta matriz foi de 0,22(1), para o Lu foi de 1,10(1) e para o Gd foi de 0,61(1). A espectroscopia de absorção mostrou que houve um alargamento das bandas em relação às bandas do LiLuF4:Nd. As secções de choque de absorção e os tempos de vida do nível 4F3/2 foram obtidos para três amostras com composições diferentes de Nd.
Title in English
STUDY OF LiGd1-xLuxF4 SOLID SOLUTIONS AIMING THE CRYSTAL GROWTH
Keywords in English
Crescimento de cristais
Fluoretos
Terras raras
Abstract in English
In this work the melting behavior of LiGd1-xLuxF4 solid solutions were studied utilizing the melting zone technique, aiming the development of new solid-state-laser matrices. Initially, crystals with composition of LiGd0.5Lu0.5F4 were systematically investigated using this method. The chemical and physical characterization of the ingots showed that this compound presents an incongruent melting behavior. Latter, some compositions of LiGd1-xLuxF4 (x = 0.60; 0.65 and 0.75) were studied to determine the composition where the LiGdF4-LiLuF4 pseudo-system starts with the formation of congruent compounds. The ingots characterization using scanning electron microscopy, energy dispersive spectrometry and X-ray diffraction, allowed to determine that the LiGd1-xLuxF4 compounds melt congruently from x values around 75 mol%. In this phase, all syntheses and zone melting processes were realized under a HF reactive atmosphere, to obtain high purity compounds. Two crystals with nominal compositions of LiGd0.25Lu0.75F4 and LiGd0.232Lu0.75Nd0.018F4 were grown from the melt by the Czochralski method, under an Ar+CF4 atmosphere. From ICP-OES concentration data, taking into account the Nd doped crystal, it was established that Lu and Gd concentrations are not constant along the crystal and there is a competition between Nd and Gd ions to be incorporated in the lattice. The calculated mean value for Nd segregation coefficient was 0.22(1), for Lu was 1.10(1) and for Gd was 0.61(1). The optical spectroscopy revealed that there is a broadening of the absorption bands in comparison with that of LiLuF4:Nd. The absorption cross sections and the 4F3/2 level lifetime were obtained for three samples with different Nd compositions. vii SUMÁRIO
 
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Publishing Date
2009-09-23
 
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